WO2018181608A1 - リチウム回収方法 - Google Patents

リチウム回収方法 Download PDF

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Publication number
WO2018181608A1
WO2018181608A1 PCT/JP2018/013029 JP2018013029W WO2018181608A1 WO 2018181608 A1 WO2018181608 A1 WO 2018181608A1 JP 2018013029 W JP2018013029 W JP 2018013029W WO 2018181608 A1 WO2018181608 A1 WO 2018181608A1
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Prior art keywords
lithium
extraction process
solvent
extraction
solution
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PCT/JP2018/013029
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English (en)
French (fr)
Japanese (ja)
Inventor
淳一 荒川
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Ｊｘ金属株式会社
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Priority to CA3058314A priority Critical patent/CA3058314C/en
Priority to EP18778276.8A priority patent/EP3604570B1/en
Priority to US16/499,170 priority patent/US11434545B2/en
Priority to CN201880022555.2A priority patent/CN110494576B/zh
Priority to KR1020197031233A priority patent/KR102282701B1/ko
Publication of WO2018181608A1 publication Critical patent/WO2018181608A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B47/00—Obtaining manganese
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

Definitions

  • the present invention relates to a method for recovering lithium by separating sodium from a lithium-containing solution containing lithium ions and sodium ions, and in particular, for recovering metal from lithium ion battery scrap, etc. It proposes the technology that can be obtained.
  • lithium-ion battery scraps are roasted to remove harmful electrolytes, then crushed and sieved in order, and then placed under a sieve.
  • the obtained powdered battery powder is added to the leaching solution and leached, and lithium, nickel, cobalt, manganese, iron, copper, aluminum and the like which can be contained therein are dissolved in the solution.
  • iron, copper, aluminum, etc. are removed sequentially or simultaneously among each metal element melt
  • the leached solution is subjected to multiple stages of solvent extraction or neutralization according to the metal to be separated, and further, back extraction, electrolysis, Apply carbonation and other treatments. Thereby, a lithium-containing solution containing lithium ions is obtained.
  • the lithium-containing solution thus obtained can be recovered as lithium carbonate by performing carbonation by adding carbonate, blowing carbon dioxide gas, or the like. Generally done.
  • Patent Document 1 discloses that the pH of an aqueous solution containing lithium ions is adjusted to a pH range of 4 to 10 according to the acidic solvent extractant used for extraction of lithium ions, After extracting lithium ions by contact, the solvent extractant is brought into contact with an aqueous solution having a pH of 3.0 or less to reversely extract lithium ions, and the above-described back extraction operation is repeated using the obtained lithium ion aqueous solution to remove lithium ions. It is described that lithium ions are recovered as solid lithium carbonate by concentrating and mixing the obtained high-concentration lithium ion aqueous solution with a water-soluble carbonate in a state kept at 50 ° C. or higher.
  • the lithium-containing solution as described above may contain a lot of sodium ions due to, for example, the addition of sodium hydroxide for the purpose of adjusting pH.
  • sodium is contained in the lithium carbonate, so that it is necessary to purify lithium carbonate to obtain lithium carbonate containing lithium in high quality.
  • the burden was large.
  • the back extract is a sulfuric acid type, sodium sulfate may be precipitated, and process troubles such as piping blockage may occur.
  • the present invention has been made paying attention to such problems, and an object thereof is to provide a lithium recovery method capable of efficiently recovering high-purity lithium from a lithium-containing solution containing lithium ions and sodium ions. It is to provide.
  • the lithium recovery method of the present invention is a method for recovering lithium by separating sodium from a lithium-containing solution containing lithium ions and sodium ions, and includes a first extraction process, a second extraction process, and a third extraction process.
  • a solvent extraction process comprising at least a three-stage extraction process having an extraction process and a lithium back-extraction process for back-extracting lithium ions from the solvent that has undergone at least the three-stage extraction process.
  • the first extraction process, the second extraction process, and the third extraction process are performed in the order, and the solution as the lithium-containing solution is subjected to the processes in the order opposite to the order of the solvent. .
  • lithium ions and sodium ions in the solution are extracted in each of the extraction processes from the first extraction process to the final extraction process excluding the final extraction process. It is preferable to extract the lithium ions in the solution into the solvent and back extract the sodium ions in the solvent into the solution in the final extraction process.
  • the pH of the final extraction process in the extraction process of at least three stages is 3.5 to 4.5.
  • the pH of the first extraction process is set to 6.0 to 6.5 in at least three extraction processes, and the final extraction stage from the second extraction process to the final extraction stage.
  • the pH of the extraction process excluding the extraction process is preferably 5.5 to 6.0.
  • the pH of the lithium-containing solution can be 2.0 to 7.0.
  • the molar ratio of the sodium concentration to the lithium concentration in the lithium-containing solution is preferably 2 to 100.
  • the lithium recovery method of the present invention further includes a nickel separation step for separating nickel from a solution containing lithium and nickel prior to the solvent extraction step, and the lithium-containing solution is obtained in the nickel separation step. can do.
  • nickel separation step nickel can be separated by solvent extraction, and a carboxylic acid-based extractant can be used for this solvent extraction.
  • the lithium-containing solution may further contain nickel ions
  • the back-extracted solution obtained in the lithium back-extraction process may contain lithium ions and nickel ions.
  • the neutralization step of neutralizing the post-extraction solution to remove nickel and after the neutralization step, carbonation to obtain lithium carbonate by carbonation from the post-neutralization solution It is preferable to further include a process.
  • the lithium-containing solution is preferably obtained by treating lithium ion battery scrap.
  • the treatment for lithium ion battery scrap can include a leaching step of leaching the lithium ion battery scrap and a recovery step of recovering the metal dissolved in the solution after leaching by solvent extraction.
  • the solvent undergoes each process in the order of the first extraction process, the second extraction process, and the third extraction process, and the solution as the lithium-containing solution is:
  • the solution as the lithium-containing solution is:
  • the lithium recovery method is a method of separating lithium from a lithium-containing solution containing lithium ions and sodium ions, and recovering lithium.
  • a solvent extraction process including a second extraction process, a third extraction process, and a lithium back extraction process for back extracting lithium ions from the solvent after the third extraction process.
  • the solvent goes through each process in the order of the first extraction process, the second extraction process, the third extraction process, and the lithium back extraction process, and the solution that is a lithium-containing solution is the third extraction process, the second extraction process.
  • Each process is performed in the order of the process and the first extraction process.
  • the target lithium-containing solution here includes at least lithium ions and sodium ions.
  • a solvent extraction step is performed on the lithium-containing solution.
  • the lithium concentration in the lithium-containing solution is, for example, 0.5 g / L to 10.0 g / L, typically 1.0 g / L to 7.0 g / L, and the sodium concentration is, for example, 1.0 g / L. L to 50.0 g / L, typically 20.0 g / L to 40.0 g / L.
  • the molar ratio of sodium concentration to the lithium concentration in the lithium-containing solution is, for example, 2 to 100, and is more effective when it is 10 or more. This embodiment can be applied to a lithium-containing solution containing sodium ions at this level.
  • the lithium-containing solution further contains nickel at 10 mg / L to 500 mg / L, typically 20 mg / L to 100 mg / L, for example when nickel remains without being separated in the previous nickel separation step. Sometimes. Thus, even if it contains nickel, the nickel can be effectively recovered from the back-extracted solution obtained in the solvent extraction step, as will be described later.
  • the lithium-containing solution may further contain cobalt, aluminum, calcium and the like at a total of 1.0 g / L or less.
  • the solvent extraction process includes an extraction process having a first extraction process, a second extraction process, and a third extraction process, and a lithium back extraction process.
  • first extraction process lithium ions contained in the lithium-containing solution are extracted into the solvent, but sodium ions can remain in the solution, and then the lithium reverse
  • lithium ions are back-extracted from the solvent to obtain a post-extraction solution from which lithium ions are contained and from which sodium ions are removed.
  • the third extraction process corresponds to the final extraction process immediately before the lithium back extraction process.
  • the solvent used in the solvent extraction step can be, for example, a phosphonate extractant (PC-88A), a phosphate ester extractant (D2EHPA), or the like.
  • PC-88A phosphonate extractant
  • D2EHPA phosphate ester extractant
  • the solvent flow and the solution flow in the first extraction process, the second extraction process, and the third extraction process are opposite to each other. More specifically, the solvent after the first extraction process is used as the solvent for the second extraction process, and the solvent after the second extraction process is used as the solvent for the third extraction process.
  • the lithium-containing solution is first used in the third extraction process, and the solution after the third extraction process is used as the solution in the second extraction process, and the solution after the second extraction process is used as the solution in the first extraction process. .
  • an unused new solvent, or a solvent after lithium is back-extracted in the lithium back-extraction process as shown in the figure, and a solution after passing through the third extraction process and the second extraction process in order.
  • solvent extraction aims at extracting the lithium ion and sodium ion in the said solution to a solvent.
  • the pH of the first extraction process is preferably 6.0 to 6.5. If the pH at this time is too high, sodium may be excessively extracted. On the other hand, if the pH is too low, there is a concern that lithium may be insufficiently extracted. Therefore, the pH of the first extraction process is more preferably 6.1 to 6.3.
  • the pH of the second extraction process is preferably equal to or lower than the pH of the first extraction process, and particularly preferably 5.5 to 6.0. If the pH in the second extraction process is too high, sodium may be excessively extracted. If the pH is too low, lithium may be insufficiently extracted. From this point of view, the pH of the second extraction process is more preferably 5.7 to 5.9.
  • solvent extraction is performed using the solvent after sequentially passing through the first extraction process and the second extraction process, and a lithium-containing solution that has not been used in the solvent extraction process.
  • sodium ions contained in the solvent move into the solution and back-extract, and lithium ions in the lithium-containing solution are extracted into the solvent.
  • the pH of the third extraction process is preferably not more than the pH of the second extraction process, and is preferably 3.5 to 4.5. If the pH of the third extraction process is too high, sodium back extraction may be insufficient. On the other hand, if the pH of the third extraction process is too low, lithium may be back-extracted. Therefore, the pH of the third extraction process is more preferably 4.0 to 4.2.
  • the lithium ion is surely included in the solvent after the third extraction process.
  • sodium ions can be effectively removed from the solvent, and lithium ions and sodium ions in the lithium-containing solution can be effectively separated.
  • Each extraction process described above can be performed based on a general method.
  • a solution (aqueous phase) and a solvent (organic phase) are contacted, and these are stirred and mixed, typically at a speed of 200 to 500 rpm, for example, for 5 to 60 minutes using a mixer, and the ions are mixed with the extractant.
  • the temperature at the time of extraction is preferably from ordinary temperature (about 15 to 25 ° C.) to 60 ° C. or less, and it is preferably carried out at 35 to 45 ° C. for reasons of extraction speed, phase separation and evaporation of organic solvent.
  • the mixed organic phase and aqueous phase are separated by a difference in specific gravity with a settler.
  • the O / A ratio volume ratio of the organic phase to the aqueous phase) depends on the content of the metal to be extracted, but is generally set to 0.1 to 10 in consideration of the operation with the mixer settler. Is preferred.
  • the solvent obtained through the third extraction process is mixed with a back extract such as sulfuric acid or hydrochloric acid, and stirred by a mixer or the like at a speed of 200 to 500 rpm, for example, for 5 to 60 minutes. be able to. It is preferable to use sulfuric acid as the back extract.
  • the acid concentration of the back extract is preferably adjusted to 0.05 to 200 g / l (pH: ⁇ 0.6 to 3.0) in order to effectively back extract lithium ions in the solvent. It is more preferable to adjust to 5 to 15 g / l (pH: 0.5 to 1.5).
  • the temperature of back extraction can be from room temperature to 60 ° C., and it is preferably carried out at 35 to 45 ° C. for reasons of back extraction speed, phase separation, and evaporation of the organic solvent.
  • the liquid after back extraction obtained in the lithium back extraction process contains lithium ions at a high concentration, but sodium ions are almost removed.
  • the lithium concentration in the solution after back extraction is preferably 5.0 g / L to 30.0 g / L, more preferably 10.0 g / L to 20.0 g / L.
  • the sodium concentration in the solution after back extraction is preferably 60.0 g / L or less, more preferably 40.0 g / L or less. Thereby, high purity lithium carbonate can be obtained in the carbonation step described later.
  • the back-extracted solution can be repeatedly used as a back-extracted solution in the lithium back-extraction process after recovering lithium contained therein, as will be described later.
  • the extraction process requires at least three stages of the first extraction process, the second extraction process, and the third extraction process.
  • the solvent will go through each process in ascending order from the first extraction process, while the solution will descend from the last extraction process before the lithium back extraction process (that is, the reverse of the solvent order). It is assumed that it goes through each process in order.
  • the pH of the extraction process from the second extraction process to the final extraction process, excluding the final extraction process is 5.5 to 6.0, particularly 5.7 to 5.
  • the second extraction process excluding the fourth extraction process, which is the final stage, of the second extraction process, the third extraction process, and the fourth extraction process and The pH of the third extraction process is preferably 5.5 to 6.0, more preferably 5.7 to 5.9.
  • the lithium ion and sodium ion in the solution are used as a solvent in each of the first extraction process to the third extraction process excluding the fourth extraction process which is the final stage.
  • Ni neutralization process When nickel ions are contained in the lithium-containing solution, the nickel ions are extracted and back-extracted together with lithium ions in the solvent extraction step, and thus are contained in the solution after back extraction. In this case, in order to separate nickel from the solution after back extraction, a neutralization step can be performed. Since nickel ions contained in the lithium-containing solution are concentrated together with lithium ions in the solvent extraction step, the nickel concentration in the solution after back extraction is, for example, 200 mg / L to 5000 mg / L, typically 500 mg / L to 3000 mg / L. L. When the lithium-containing solution does not contain nickel ions, the neutralization step can be omitted.
  • the neutralization step by adding alkali to the acidic back-extracted solution, the back-extracted solution is neutralized and nickel is recovered as a solid.
  • alkali at this time include sodium hydroxide and calcium hydroxide.
  • the pH of the back-extracted solution obtained in the above-described lithium back-extraction process is, for example, 0.5 to 1.5.
  • the pH is adjusted to 10 to 10 by adding alkali to the back-extracted solution. 13 is preferable.
  • the liquid temperature in the neutralization step can be normal temperature, and the mixture can be stirred at a predetermined speed and time after the addition of alkali. Thereby, the nickel concentration in the liquid after back extraction can be lowered to about 10 mg / L or less.
  • the neutralized solution obtained by removing nickel in the neutralization step can be subjected to a carbonation step in order to recover lithium contained therein.
  • a carbonation step in order to recover lithium contained therein.
  • carbonate by adding carbonate to the post-neutralization solution or blowing carbon dioxide gas, lithium ions in the post-neutralization solution are recovered as lithium carbonate.
  • the liquid temperature is set within a range of 20 ° C. to 50 ° C., and stirring is performed as necessary to maintain a predetermined time.
  • the carbonate added to the solution after neutralization include sodium carbonate and ammonium carbonate, and sodium carbonate is preferred from the viewpoint of recovery.
  • the amount of carbonate added can be, for example, 1.0 to 1.7 times, preferably 1.2 to 1.5 times the Li molar amount.
  • the amount of carbon dioxide added can be, for example, 1.0 to 1.7 times, preferably 1.2 to 1.5 times the Li molar amount.
  • the pH of the solution after neutralization during carbonation is preferably relatively high, 10-13. If carbonate is added in a state where the pH is low, carbon dioxide gas is lost, so there is a concern that the reaction efficiency may be reduced.
  • the pH of the neutralized solution can be adjusted to the above range.
  • the lithium carbonate thus obtained has a high purity without containing sodium by removing sodium in the solvent extraction step described above.
  • the lithium quality of lithium carbonate is preferably 17% or more, more preferably 18% or more.
  • lithium carbonate can be purified in order to obtain higher quality lithium carbonate. This purification can be performed by a generally known method.
  • the present invention can be applied to various lithium-containing solutions as long as they contain sodium ions.
  • the present invention is used in mobile phones and other various electronic devices and has a product life, manufacturing failure, etc. It is preferable to apply to the lithium containing solution obtained by processing the lithium ion battery scrap discarded for the reasons described above.
  • the lithium ion battery scrap is subjected to roasting treatment and chemical treatment as necessary, and is crushed and sieved to obtain battery powder.
  • the battery components are dissolved by acid leaching.
  • copper which can be contained in the lithium ion battery scrap can be removed by solid-liquid separation after leaching without dissolving.
  • a recovery process including multiple stages of solvent extraction is performed on the liquid after leaching, and iron, aluminum, manganese, cobalt, and nickel are sequentially separated to obtain a lithium-containing solution.
  • the lithium-containing solution thus obtained may contain nickel when nickel is not completely separated in the nickel separation step by solvent extraction as the previous step.
  • sodium hydroxide is added to adjust the pH, the lithium-containing solution contains sodium ions.
  • Example 1 The first extraction process to the third extraction process and the Li back extraction process are performed, the pH of the first extraction process is 6.0, the pH of the second extraction process is 5.8, and the pH of the third extraction process is 4 .0.
  • the pre-extraction solution (lithium-containing solution) has a Li concentration of 1.5 g / L and a Na concentration of 45 g / L. From this pre-extraction solution, a Li concentration of 12.2 g / L and a Na concentration of 47.3 g / L are back-extracted. A post-solution was prepared.
  • the Na / Li molar ratio of the pre-extraction solution is 9.09
  • the Na / Li molar ratio of the post-extraction solution is 1.173
  • the ratio of the Na concentration to the Li concentration is about 0.13.
  • the concentration of can be sufficiently reduced.
  • Example 2 The first extraction process to the third extraction process and the Li back extraction process are performed, the pH of the first extraction process is set to 6.0, the pH of the second extraction process is set to 5.9, and the pH of the third extraction process is set to 4 .8.
  • the Li concentration of the pre-extraction solution (lithium-containing solution) is 1.1 g / L, and the Na concentration is 36 g / L. From this pre-extraction solution, the Li concentration is 8.5 g / L and the Na concentration is 46.0 g / L. A post-solution was prepared.
  • the Na / Li molar ratio of the pre-extraction liquid is 9.90
  • the Na / Li molar ratio of the liquid after back extraction is 1.62
  • the ratio of the Na concentration to the Li concentration is about 0.16.
  • the Na concentration did not decrease as much as in Example 1.

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PCT/JP2018/013029 2017-03-30 2018-03-28 リチウム回収方法 WO2018181608A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CA3058314A CA3058314C (en) 2017-03-30 2018-03-28 Lithium recovery method
EP18778276.8A EP3604570B1 (en) 2017-03-30 2018-03-28 Lithium recovery method
US16/499,170 US11434545B2 (en) 2017-03-30 2018-03-28 Lithium recovery method
CN201880022555.2A CN110494576B (zh) 2017-03-30 2018-03-28 锂回收方法
KR1020197031233A KR102282701B1 (ko) 2017-03-30 2018-03-28 리튬 회수 방법

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JP2017068967A JP6599396B2 (ja) 2017-03-30 2017-03-30 リチウム回収方法

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KR102551138B1 (ko) * 2021-07-19 2023-07-04 코스모화학 주식회사 리튬을 함유하는 여액으로부터 리튬화합물을 회수하는 방법
CN113493871A (zh) * 2021-09-08 2021-10-12 金驰能源材料有限公司 一种解决p507钴萃取系统中镍镁萃取过萃的方法
WO2024181818A1 (ko) * 2023-03-02 2024-09-06 서강대학교산학협력단 리튬 함유 재료로부터 리튬을 추출하는 방법

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007122885A (ja) * 2005-10-25 2007-05-17 Sumitomo Metal Mining Co Ltd リチウムイオン電池からの有価金属回収方法
JP2009193778A (ja) * 2008-02-13 2009-08-27 Nippon Mining & Metals Co Ltd Ｃｏ，Ｎｉ，Ｍｎ含有リチウム電池滓からの有価金属回収方法
JP4581553B2 (ja) 2004-08-20 2010-11-17 住友金属鉱山株式会社 リチウムの回収方法
JP2011011961A (ja) * 2009-07-06 2011-01-20 Jx Nippon Mining & Metals Corp リチウムイオン２次電池回収物からの炭酸リチウムの製造方法
JP2014162982A (ja) * 2013-02-27 2014-09-08 Jx Nippon Mining & Metals Corp 金属混合溶液からの金属の分離回収方法
JP2016060926A (ja) * 2014-09-16 2016-04-25 ソルベイ日華株式会社 金属の分離方法

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3707577A (en) * 1971-03-08 1972-12-26 Exxon Research Engineering Co Separation of aromatics
JP5014394B2 (ja) 2009-09-29 2012-08-29 Ｊｘ日鉱日石金属株式会社 ニッケルとリチウムの分離回収方法
CN102002595B (zh) * 2010-12-24 2013-04-24 佛山市邦普循环科技有限公司 一种废旧电池中锂的回收方法
JP5857572B2 (ja) * 2011-09-16 2016-02-10 住友金属鉱山株式会社 有価金属回収方法
US10522884B2 (en) * 2012-04-04 2019-12-31 Worcester Polytechnic Institute Method and apparatus for recycling lithium-ion batteries
CN103384002B (zh) * 2012-05-04 2017-07-07 湖南科飞特高新技术有限公司 一种利用镍钴渣制备电子三元材料前驱体的方法
JP5898021B2 (ja) * 2012-09-11 2016-04-06 株式会社日立製作所 リチウムイオン電池の再資源化方法、およびその装置
CN104388677A (zh) * 2014-12-02 2015-03-04 中国科学院青海盐湖研究所 一种锂萃取体系再生的方法
CN105483382B (zh) 2015-12-04 2017-06-23 清华大学 含镍钴锰的废电池材料浸出液的分离回收方法
CN105742744B (zh) * 2016-03-03 2017-10-31 中南大学 一种从废旧锂离子电池回收过程产生的含锂废液中提取锂的方法
CN106521159B (zh) * 2016-10-11 2017-12-15 天津科技大学 基于含Fe(III)的萃取体系萃取卤水中锂及回收利用Fe(III)的方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4581553B2 (ja) 2004-08-20 2010-11-17 住友金属鉱山株式会社 リチウムの回収方法
JP2007122885A (ja) * 2005-10-25 2007-05-17 Sumitomo Metal Mining Co Ltd リチウムイオン電池からの有価金属回収方法
JP2009193778A (ja) * 2008-02-13 2009-08-27 Nippon Mining & Metals Co Ltd Ｃｏ，Ｎｉ，Ｍｎ含有リチウム電池滓からの有価金属回収方法
JP2011011961A (ja) * 2009-07-06 2011-01-20 Jx Nippon Mining & Metals Corp リチウムイオン２次電池回収物からの炭酸リチウムの製造方法
JP2014162982A (ja) * 2013-02-27 2014-09-08 Jx Nippon Mining & Metals Corp 金属混合溶液からの金属の分離回収方法
JP2016060926A (ja) * 2014-09-16 2016-04-25 ソルベイ日華株式会社 金属の分離方法

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